AbstractAdvances in electrocatalysis require the development of high specific surface area materials with high electron conductivity. In this study, a series of MCNTs@MoS2(1‐x)Se2x nanocomposites has been prepared for application in catalytic hydrogen evolution. A uniform growth of MoS2(1‐x)Se2x nanoflower spheres on MCNTs has been achieved, circumventing stacking and aggregation. The introduction of the conducting material accelerated the electron transport rate in the electrode reaction. Structural characterization has confirmed that S doping increased the specific surface area of the catalyst, exposing more edge defects. As a result, the MCNTs@MoS2(1‐x)Se2x nanocomposites exhibited enhanced catalytic activity. Electrochemical tests have established that MCNTs@MoS1.5Se0.5 possessed the lowest overpotential (146 mV) at a current density of 10 mA/cm2 with the smallest Tafel slope (45.1 mV/dec).
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